Hydrogen Peroxide → HCID 14404512, compound
Reaction equation
[CH2:1]([S:8][CH2:9][CH2:10][CH2:11][Cl:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:13]O>C(O)(=O)C.O>[CH2:1]([S:8]([CH2:9][CH2:10][CH2:11][Cl:12])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
1.2 g of 1-benzylthio-3-chloro-n-propane, synthesized by ◯1 of Synthesis Example 2 was dissolved in 50 ml of acetic acid, and 8.7 g of 35% aqueous hydrogen peroxide was added thereto dropwise under stirring below 10° C. After that, it was warmed gradually to room temperature again, then stirred further for 4 hours. The reaction mixture was poured in 300 ml of iced water, and extracted 2 times by each 150 ml of methylene chloride. The methylene chloride layer was washed 2 times with 5% aqueous solution of sodium hydroxide, followed by water, and dried over anhydrous magnesium sulfate. A colorless solid residue was obtained by distilling off methylene chloride. It was washed by n-hexane to give 12.6 g (yield: 96.9%) of the object 1-benzylsulfinyl-3-chloro-n-propane as a colorless crystal. m.p. 70° to 71° C.
Workup
- stirringstirred further for 4 hours
- extractionextracted 2 times by each 150 ml of methylene chloride
- washThe methylene chloride layer was washed 2 times with 5% aqueous solution of sodium hydroxide
- dry with materialdried over anhydrous magnesium sulfate
- customA colorless solid residue was obtained
- distillationby distilling off methylene chloride
- washIt was washed by n-hexane
Sources & evidence
- ORD record
- ord-1082503d5b4841d3bc51b34d348d45fb
- Source dataset
- uspto-grants-1990_06
- Patent number
- US04931474
Reaction notes
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